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Dionex IONPAC AG9-SC GUARD COLUMN Product Manual

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Summary of Contents for Dionex IONPAC AG9-SC GUARD COLUMN

  • Page 1 ® IonPac AG9-SC ® IonPac AS9-SC...
  • Page 2 Page 1 of 28 PRODUCT MANUAL for the ® IONPAC AG9-SC GUARD COLUMN (4 x 50 mm, P/N 043186) ® IONPAC AS9-SC ANALYTICAL COLUMN (4 x 250 mm, P/N 043185) ©DIONEX Corporation, 2008 Document No. 034656 Revision 06 November 2008...

  • Page 3: Table Of Contents

    The Sample Concentrator ............................6 The Injection Loop ..............................6 3.3.1 The 4-mm System Injection Loop, 10 - 50 μL ......................7 The IonPac AG9-SC Guard Column ........................7 Installing the Anion Trap Column, ATC-3 ......................7 Eluent Storage ................................8 The Anion Self-Regenerating Suppressor, ASRS®...
  • Page 4 IonPacAS9-SC 034656-06 Page 3 of 28 Eluents that Contain Solvents ..........................13 Regenerant Preparation for the AMMS III ....................... 13 The Sample Concentrator ............................ 14 SECTION 5 - EXAMPLE APPLICATIONS................. 15 Production Test Chromatogram .......................... 16 Inorganic Anions Including Chlorate and Chlorite ................... 17 Resolution of Low-Concentration Analytes - EPA Water Matrix ..............

  • Page 5: Section 1 - Introduction

    Always remember that assistance is available for any problem that may be encountered during the shipment or operation of DIONEX instrumentation and columns through the DIONEX North America Technical Call Center at 1-800-DIONEX-0 (1-800-346-6390) or through any of the DIONEX Offices listed in, “DIONEX Worldwide...

  • Page 6: Section 2 - The Ion Chromatography System

    Either the TS-1 with the TS-2 can be used with the CDM-2 or the CDM-3. Do not use the TS-2 or the TS-1 with the ED40/ED50 or the CD20/CD25. DIONEX Back Pressure Regulator 75 psi rating (P/N 039760, 046480) or Tubing (see Table 3) Ensure 50-75 psi back pressure.

  • Page 7: Section 3 - Installation

    3.1.1 System Requirements for 4-mm Operation The IonPac AS9-SC 4-mm Guard and Analytical Columns are designed to be run on the following DIONEX Ion Chromatographs equipped with suppressed conductivity detection. Isocratic analyses at flow rates of 0.5 mL/min or greater can be performed on a GS50/GP50/GP40/IP25, Gradient Pump Module (GPM-2) or an Advanced Gradient Pump (AGP) with standard (1/8"...

  • Page 8: The 4-Mm System Injection Loop, 10 - 50 Μl

    The IonPac AG9-SC Guard Column An IonPac AG9-SC Guard Column is normally used with the IonPac AS9-SC Analytical Column. Retention times will increase by approximately 20% when a guard column is placed in-line prior to the analytical column. A guard is placed prior to the analytical column to prevent sample contaminants from eluting onto the analytical column.

  • Page 9: Eluent Storage

    To minimize the baseline shift when performing an analysis that requires a borate gradient, a high regenerant flow rate (10 - 15 mL/min) is required. To save regenerant preparation time and reduce regenerant consumption and waste, DIONEX recommends using an AutoRegen® Accessory (P/N 039594).

  • Page 10: Using Displacement Chemical Regernation (Dcr) With The Chemical Suppression Mode

    3.11 Using Displacement Chemical Regernation (DCR) with the Chemical Suppression Mode DIONEX recommends using the Displacement Chemical Regeneration (DCR) Mode for chemical suppression using sulfuric acid and the Anion MicroMembrane Suppressor (AMMS III). See the DCR kit manual, Document P/N 031664, for details.

  • Page 11: Section 4 - Operations

    Low trace impurities and low particle levels in eluents also help to protect your ion exchange columns and system components. DIONEX cannot guarantee proper column performance when the quality of the chemicals, solvents and water used to prepare eluents has been compromised.

  • Page 12: Deionized Water

    Page 11 of 28 solvents will usually ensure that your chromatography is not affected by ionic impurities in the solvent. Currently at DIONEX, we have obtained consistent results using High Purity Solvents manufactured by Burdick and Jackson and OPTIMA® Solvents by Fisher Scientific.

  • Page 13: Preparation Of Carbonate Eluents

    D. AS4A Sodium Carbonate/Bicarbonate Concentrate (100X) 0.18 M Na /0.17 M NaHCO 1. Order DIONEX P/N 039513 or 2. Thoroughly dissolve 19.078 g of Na and 14.282 g of NaHCO in 700 mL of deionized water with a specific resistance of 18.2 megohm-cm.

  • Page 14: Eluents That Contain Solvents

    IonPacAS9-SC 034656-06 Page 13 of 28 Eluents that Contain Solvents When mixing solvents with water remember to mix solvent with water on a volume to volume basis. For example, if a procedure requires an eluent of 90% acetonitrile, prepare the eluent by adding 900 mL of acetonitrile to an eluent reservoir. Then add 100 mL of deionized water to the acetonitrile in the reservoir.

  • Page 15: The Sample Concentrator

    IonPacAS9-SC 034656-06 Page 14 of 28 The Sample Concentrator The Low Pressure Trace Anion Concentrator Column (TAC-LP1, P/N 046026), the Trace Anion Concentrator Column (TAC-2, P/N 043101), the Anion MicroConcentrator, AMC-1, (P/N 051760) or the IonPac AG9-SC 4-mm Guard Column can be used for trace anion concentration work required in high purity water analysis.

  • Page 16: Section 5 - Example Applications

    IonPacAS9-SC 034656-06 Page 15 of 28 SECTION 5 - EXAMPLE APPLICATIONS Before attempting any of the following example applications, take the time to ensure that your system is properly configured. Ensure that all of the eluents have been made from high purity reagents and deionized water. All water used in the preparation of eluents should be degassed, deionized water.

  • Page 17: Production Test Chromatogram

    IonPacAS9-SC 034656-06 Page 16 of 28 Production Test Chromatogram Isocratic elution of anions on the IonPac AS9-SC Analytical Column has been optimized utilizing a carbonate/bicarbonate eluent. By using this eluent, mono- and divalent anions, including oxyhalides can be isocratically separated and quantitated in a single injection.

  • Page 18: Inorganic Anions Including Chlorate And Chlorite

    IonPacAS9-SC 034656-06 Page 17 of 28 Inorganic Anions Including Chlorate and Chlorite Separation and elution of anions on the IonPac AS9-SC Analytical Column has been optimized utilizing a carbonate/bicarbonate eluent. By using this eluent, monovalent and divalent anions can be isocratically separated and quantitated in a single injection. The carbonate/bicarbonate mixture allows the strength of the eluent, and thus the selectivity of the system to be changed by varying the HCO ratio.

  • Page 19: Resolution Of Low-Concentration Analytes - Epa Water Matrix

    IonPacAS9-SC 034656-06 Page 18 of 28 Resolution of Low-Concentration Analytes - EPA Water Matrix The following example demonstrates the separation of sample analytes having highly variable concentrations. Setting the flow rate at 1.0 mL/min allows for increased resolution of very low concentration analytes such as bromate, chlorite, and chlorate in the following EPA water matrix sample.

  • Page 20: Varying The Eluent System - 22 Mm Borate

    IonPacAS9-SC 034656-06 Page 19 of 28 Varying the Eluent System - 22 mM Borate The borate eluent gives the same elution order as the carbonate eluent traditionally used on the IonPac AS9. However, since the borate anion is a “weaker” eluent ion, higher concentrations are required to achieve the same elution time. The advantage of the borate eluent is increased resolution of early eluting ions.

  • Page 21: Varying The Eluent System - 10 Mm Borate With Column Purge

    IonPacAS9-SC 034656-06 Page 20 of 28 Varying the Eluent System - 10 mM Borate with Column Purge A low concentration of borate is used to improve resolution of early eluting peaks. This is particularly beneficial when quanititating chlorite and bromate at sub-ppm levels in the presence of high amounts of fluoride and chloride. High amounts of nitrate, phosphate, or sulfate can be rapidly removed from the column using a step change to a higher borate concentration.

  • Page 22: Section 6 - Troubleshooting Guide

    For more information on problems that originate with the Ion Chromatograph (IC) or the suppressor refer to the Troubleshooting Guide in the appropriate operator’s manual. If you cannot solve the problem on your own, call the DIONEX Worldwide Office nearest you (see, DIONEX Worldwide Offices).

  • Page 23: High Background Or Noise

    IonPacAS9-SC 034656-06 Page 22 of 28 IonPac AS9-SC 4-mm Columns Part (P/N) Analytical Column 043185 Guard Column 043186 Bed Support Assembly 042955 End Fitting 052809 CAUTION If the column tube end is not clean when inserted into the end fitting, particulate matter may obstruct a proper seal between the end of the column tube and the bed support assembly.

  • Page 24: A Contaminated Guard Or Analytical Column

    IonPacAS9-SC 034656-06 Page 23 of 28 and varying baseline will result. In this case the AMMS III or the ASRS-ULTRA will need to be serviced as outlined in the AMMS III manual (see Document No. 031727, Product Manual for the Anion MicroMembrane Suppressor III, the AMMS III or Document No.

  • Page 25: Contaminated Hardware

    The original column capacity should be restored by this treatment, since the contaminants should be eluted from the column. If you need assistance in solving resolution problems, contact the nearest DIONEX Worldwide Office (see, DIONEX Worldwide Offices) 6.2.6 A Contaminated Anion Self-Regenerating Suppressor, ASRS-ULTRA...

  • Page 26: Contaminated Anion Micromembrane Suppressor, Amms Iii

    IonPacAS9-SC 034656-06 Page 25 of 28 D. Disconnect the liquid line from the ASRS-ULTRA ELUENT OUT port to the cell at the cell fitting and reconnect it to the REGEN IN port. E. Connect a temporary line from the priming block or the low-pressure tee on the isocratic or gradient pump to a container with a solution of 0.2 M oxalic acid.
  • Page 27 IonPacAS9-SC 034656-06 Page 26 of 28 C. If you are running in the AutoSuppression External Water Mode, turn off the external water and disconnect the external water line from the AAES REGEN IN port. D. Disconnect the liquid line from the AAES ELUENT OUT port to the cell at the cell fitting and reconnect it to the REGEN IN port.

  • Page 28: Loss Of Front End Resolution

    (broad) peaks can show up at unexpected times. Clean the column as indicated in “Column Care.” B. If you need assistance in determining the best way to clean strongly retained solutes in your specific sample matrix from the IonPac AS9-SC columns, contact the nearest DIONEX Worldwide Office (see, DIONEX Worldwide Offices).
  • Page 29 Small baseline disturbances at the beginning or at the end of the chromatogram can be overlooked as long as they do not interfere with the quantification of the peaks of interest. For DX-300 systems equipped with a Rheodyne Microinjection Valve, Model 9126 (DIONEX P/N 044697), consult the accompanying manual for service instructions.
  • Page 30 IonPac AS9-SC Column Care Document No. 034656C06 Page 1 of 4 RECOMMENDED OPERATION PRESSURES Operating a column above its recommended pressure limit can cause irreversible loss of column performance. The maximum recommended operating pressure for IonPac AS9-SC columns is 4,000 psi. COLUMN START-UP The column is shipped in 2.0 mM Na /0.75 mM NaHCO...
  • Page 31 BASE-SOLUBLE CONTAMINANTS WARNING Do not use the standard NaOH procedure described in other DIONEX documentation for base cleanup of IonPac AS9-SC/AG9-SC Columns. This procedure will destroy IonPac AS9-SC/AG9-SC Columns A. Prepare a 500 mL solution of 200 mM Na /75 mM NaHCO (see Section 4.1, Preparation of Eluent Concentrates).
  • Page 32 WARNING Do not use the standard HCl procedure described in other DIONEX documentation for base cleanup of IonPac AS9-SC/AG9-SC Columns. This procedure will destroy IonPac AS9-SC/AG9-SC Columns A. Prepare a 500 mL cleanup solution of 100 mM oxalic acid/50 mM NaOH (pH 2.5 to 3.0) by dissolving 6.2 g of oxalic acid dihydrate with 4.2 g (2.6 mL) of 50% w/w sodium hydroxide concentrate solution with 400 ml of deionized water...
  • Page 33 IonPac AS9-SC Column Care Document No. 034656C06 Page 4 of 4 ORGANIC CONTAMINANTS A. Prepare a two bottles with approximately 500 mL each of the following two eluents. In the first bottle (E1) place 100% acetonitrile. In the second bottle (E2) make a 1M solution of NaCl using deionized water having a specific resistance of 18.2 megohm-cm and then adjust the pH of the solution to pH 2.0 using HCl.

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